Effects of pyrolysis processes on the microstructures and mechanical properties of Cf/SiC composites using polycarbosilane

Three-dimensional braided carbon fiber reinforced silicon carbide composites (3D-B C_f/SiC) were prepared through eight cycles of vacuum infiltration of polycarbosilane (PCS) and subsequent pyrolysis under an inert atmosphere. The influences of heating rate and pyrolysis temperature on the microstructure and mechanical properties of C_f/SiC were discussed. It was found that the heating rate had great effect on the mechanical properties of C_f/SiC composites. With the increase of heating rate, the density of C_f/SiC composites increased and the interfacial bonding was weakened. As a result, the flexural strength of C_f/SiC was enhanced from 145 to 480 MPa when the heating rate was increased from 0.5 to 15 °C/min. The results showed that the flexural strength of the C_f/SiC composites fabricated at a heating rate of 15 °C/min could be increased from 480 to 557 MPa if the pyrolysis temperature of the sixth cycle was elevated from 1200 to 1600 °C, which was also attributed to the desirable interfacial structure and increased density. When tested at 1300 °C in vacuum, the C_f/SiC showed higher flexural strength (680 MPa) than that (557 MPa) at room temperature.     

Comparison of oxidation behaviors of 3D C/PyC/SiC and SiC/PyC/SiC composites in an O2-Ar atmosphere

Oxidation behaviors of three-dimensional woven C/PyC/SiC and SiC/PyC/SiC prepared by CVI processing were investigated in an O₂-Ar atmosphere at 600 °C, 900 °C and 1200 °C, respectively, by using thermogravimetric analysis. After machining, both composites should be protected by CVD SiC coating, which was demonstrated effectively in improving the oxidation resistance of both composites. The oxidation behavior of SiC/PyC/SiC was different from that of C/PyC/SiC. The oxidation kinetics of C/PyC/SiC was controlled by the rate of the reaction between carbon and oxygen at 600 °C and by the oxygen diffusion through the coating microcracks at 900 °C. The oxidation kinetics of SiC/PyC/SiC at both 600 °C and 900 °C were assumed to be controlled by the oxygen diffusion through channels of coating and matrix defects and looped pipelines instead of PyC interphase. At 1200 °C, the oxidation was controlled by oxygen diffusion through the SiO₂ scale, which took place mainly on the surfaces of both composites.     

基于酚醛树脂的碳/碳复合材料在高温分解过程的微结构演变

采用热压成型方法制备碳/ 酚醛树脂预制体, 再经高温碳化得到开气孔率为27 %、密度约1. 27 g/ cm3并具有预期孔隙结构的碳/ 碳复合材料。研究了200～900 ℃预制体转化为碳/ 碳复合材料过程中, 材料的密度、开气孔率、失重率、以及内部微观结构随温度的变化。分析了材料在高温分解过程中微观结构演变规律。结果表明,酚醛树脂主要在400～700 ℃大量分解, 其分解速率约为其余温度范围的4 倍, 该温度范围失重率增加了14 %、开气孔率增加了18 %。在高于400 ℃时形成大量裂纹与孔隙, 随着温度升高裂纹增多并进一步扩展, 900 ℃碳化后形成一种连通的特征性微观裂缝网格模式。高温分解后碳/ 碳复合材料中总孔容约0. 17 cm3 / g , 其中81 %的孔隙半径在122. 190～2. 440μm 范围内。      

三向正交碳纤维增强纳米碳化硅生物复合材料的制备和力学性能

碳纤维增强的纳米碳化硅陶瓷基复合材料力学性能优良,且具有一定的生物相容性,因此可作为一种新型的可取代钛合金的全尺寸整体人工骨骼。研究了具有三向正交结构的T300和M30碳纤维预制体对C/SiC复合材料制备过程和抗弯强度的影响规律。以聚碳硅烷为先驱体,以二乙烯基苯为溶剂和交连剂,采用聚合物浸渍热解法制备了C/SiC复合材料,采用阿基米德排水法测量其密度和气孔率,采用三点抗弯法测量其抗弯强度。M30 C/SiC抗弯强度比T300 C/SiC高6.7％,表明碳纤维弹性模量对复合材料基体开裂强度有显著影响,并通过增加纤维径向强度以及承担载荷的比例提高了复合材料的断裂强度。      

Influence of CVI treatment of carbon fibers on the electromagnetic interference of CFRC composites

Short carbon fibers were treated at temperatures around 1100 °C in a furnace through chemical vapor infiltration technology. The fiber surface was observed by scanning electron microscopy. The reflectivity of electromagnetic radiation by the composites that were reinforced by surface-treated carbon fibers and by as-received ones was measured in the frequency range of 8.0–18.0 GHz. The reflectivity for different carbon fiber contents of 0.2%, 0.4%, 0.6% and 1.0 wt% was investigated. Results showed that the reflectivity of the composites that were reinforced by untreated carbon fibers tended to increase with the increasing fiber contents. The minimum reflectivity was −19.3 dB, far less than −10 dB, when the fiber content was 0.4% and there were wave-absorbing properties. However, after surface treatment, the minimum reflectivity was −8.1 dB for the same fiber content of 0.4%, indicating significant wave-reflecting properties. The achieved reflectivity values after surface treatment were generally greater than those without treatment.     

Effects of microstructure on flexural strength of biomorphic C/SiC composites

Biomorphic C/SiC composites were fabricated from different kinds of wood by liquid silicon infiltration (LSI) following a two-step process. In the first-step, the wood is converted into carbon preforms by pyrolysis in a nitrogen atmosphere. The carbon preforms are then infiltrated by silicon melt at 1,560°C under vacuum to fabricate C/SiC composites. The mechanical properties of the C/SiC composites were characterized by flexural tests at ambient temperature, 1,000, and 1,300°C, and the relationship between mechanical properties and microstructure was analyzed. The flexural strength of the biomorphic composites was strongly dependent on the properties of the carbon preforms and the degree of silicon infiltration. The flexural strength increased with increasing SiC content and bulk density of composite, and with decreasing porosity in the C/SiC composite. An analysis of fractographs of fractured C/SiC composites showed a cleavage type fracture, indicating brittle fracture behavior.     

Using phenol–formaldehyde resin as carbon source to synthesize mesoporous carbons of different pore structures

In this research communication, we performed the phenol–formaldehyde (PF) resin as an alternative carbon source and various mesostructured silicas as the nano-templates to conveniently prepare the mesoporous carbons of high surface area (850–1500 m² g⁻¹), large pore size (2.0–22.0 nm) and great pore volume (0.65–1.15 cm³ g⁻¹). It was reasonably supposed that there exist interaction matching between the negative-charged silica surface of the silica template and PF resin. Therefore, the PF oligomers could be homogeneously adsorbed into the nanochannels or cages of the mesoporous silicas via an impregnation process. Because the thermosetting PF resin only requires a simple heat treatment process at 100 °C to form the cross-linked polymeric structure, the replication of the mesostructure of the mesoporous silica template could be readily achieved without adding any polymerization catalysts.     

Multi-composition oxidation resistant coating for SiC-coated carbon/carbon composites at high temperature

This work proposes a multi-composition oxidation resistant coating for SiC-coated carbon/carbon (C/C) composites by slurry method using the mixture of Y₂O₃, ZrO₂, Al₂O₃, Si and C. XRD analysis shows that the phases of the composite coating are composed of SiC, Al₂O₃, Y₂O₃, ZrO₂, Al₄SiC₄ and Y₃Al₂(AlO₄)₃. SEM analysis of the cross section of the coating displays the microstructure with 500 μm thickness which filled the porous SiC. Oxidation test shows that, after 19 h oxidation in air at 1873 K, the weight loss of the coated SiC-C/C is only 1.76%. The oxidation of the coated C/C composites was primarily due to the reaction of C/C matrix and oxygen diffusing through the penetrable cracks and bubble holes in the coating.     

Effects of oxidation on surface stresses and mechanical properties of liquid phase pressureless-sintered SiC–AlN–Y2O3 ceramics

The understanding of the oxidation mechanism of 50 wt% SiC–50 wt% AlN composites obtained by means of pressureless sintering without the protective powder bed and with Y₂O₃ as sintering-aid were significantly improved by means of Raman spectroscopy. These analyses put in evidence that “amorphous carbon” started to be formed at 1300 °C as main effect of active oxidation of SiC. At higher temperature the crystallization process began and it was completed at 1500 °C when only graphite could be recognized. On the basis of these new evidences, oxidation effects on the mechanical properties of SiC–AlN–Y₂O₃ composites were defined. First of all, heat treatment in air was able to induce a compressive surface stress due to the volume gain associated to the oxidation of the intergranular phase. As a consequence apparent fracture toughness showed a value of 6.6 MPa m^1/2 after a heat treatment at 1300 °C, while at higher temperature effects of active oxidation caused a decreasing up to 4.7 MPa m^1/2. This toughening mechanism was also used to improve the resistance to thermal shock, which was evaluated by performing quenching tests. Furthermore, passive oxidation induced the healing of superficial flaws by means of the formation of -cristobalite. This phenomenon was assumed to be responsible for the increasing of the flexural strength.     

In situ synthesis mechanism and characterization of ZrB2–ZrC–SiC ultra high-temperature ceramics

The synthesis route, microstructure and properties of ZrB₂–ZrC–SiC composites prepared from a mixture of Zr–B₄C–Si powders by in situ reactive synthesis were investigated. The reactive path and synthesized mechanism of ZrB₂–ZrC–SiC composite were studied through series of pressureless heat treatments ranging from 800 °C to 1700 °C in argon. The in situ ZrB₂–ZrC–SiC composites were fabricated under different synthesis processing. The one with 88.4% relative density performed poorly in mechanical properties due to the occurring of self-propagating high-temperature synthesis (SHS). The fully dense ZrB₂–ZrC–SiC composite was obtained under the optimized synthesis processing without SHS reactions. Its Vickers hardness, flexural strength and fracture toughness were 20.22 ± 0.56 GPa, 526 ± 9 MPa and 6.70 ± 0.20 MPa m^1/2, respectively.     

High temperature electrical and thermal properties of the bulk carbon nanotube prepared by SPS

Bulk multi-walled carbon nanotube was prepared by spark plasma sintering at 1700 °C under a pressure of 50 MPa in vacuum. The density of the bulk sample reaches 72% of the theoretical density of the carbon nanotube, 2 g/cm³. The high temperature thermal conductivity and electrical conductivity of the bulk material were measured in the directions perpendicular and parallel to the pressure direction. Both the thermal conductivity and electrical conductivity show apparent anisotropy. The thermoelectric power has close values in the two different directions and takes positive values in the whole measured temperature range (360–840 K).     

Kinetics of chemical vapor infiltration of carbon nanofiber-reinforced carbon/carbon composites

Preforms containing 0, 5, 10, 15 and 20 wt.% carbon nanofibers (CNFs) were fabricated by spreading layers of carbon cloth, and infiltrated by using the technique of isothermal chemical vapor infiltration (ICVI) at the temperature of 1100 °C under the total pressure of 1 kPa and with the flow of the mixture of propane/nitrogen in a ratio of 13:1. The infiltration rates increased with the rising of CNF content, and after 580 h of infiltration, the achievable degree of pore filling was the highest when the CNF content was 5 wt.%, but the composite could not be densified efficiently as the CNF content ranged from 10 to 20 wt.%. An analysis of the results, based on the effective diffusion coefficient and on the in-pore deposition rates, shows that the CNFs, due to their higher aspect ratio, accelerate overgrowth at pore entrances and thus lead to incomplete pore filling.     

Photoluminescence properties of the Yb:Er co-doped Al2O3 thin film fabricated by microwave ECR plasma source enhanced RF magnetron sputtering

The Yb:Er co-doped Al₂O₃ thin film was deposited on oxidized silicon wafers by microwave ECR plasma source enhanced RF magnetron sputtering, and annealed from 800 °C to 1000 °C. The photoluminescence at 1.53 μm of thin film was obtained under room temperature. The mixture phase structure of γ and θ is observed by XRD, and the compositions of the thin film are investigated by EPMA. The maximum PL intensity was achieved with O₂:Ar at 1:1, annealing temperature at 900 °C, and experimental ratio of Yb:Er at 1:3.6. The energy transfer mechanism between Er and Yb ions is supported by theoretical analysis and experiment results.     

Effect of temperature gradients and stress levels on damage of C/SiC composites in oxidizing atmosphere

Strain response of a C/SiC composite, which is cycled with ΔT₁ of 500 °C at 50 MPa, ΔT₂ of 400 °C at 100 MPa and ΔT₃ of 300 °C at 150 MPa, was investigated. Measured thermo-elastic strain ranges are found to retain 0.209% for ΔT₁, 0.168% for ΔT₂, and 0.122% for ΔT₃, independent upon the applied stress level. Non-linear variations of thermal cycling creep strain can reflect damage evolutions of the composites by changing its rate, which depends on temperature gradient and applied stress. After 104 thermal cycles, strength, modulus, and failure strain of the composites retain 60.29%, 84.2%, and 59% of the initial properties, respectively. The coating cracks of the cycled specimens are observed to be perpendicular to the applied stresses and arranged at relatively regular spacing, through which the fibers are oxidized superficially.     

The influence of silicon on carbon redistribution in steel weldments

Carbon redistribution was measured in ST1/ST2 Fe-2.5Si-0.8C/Fe-0.32Si-0.49C steel weldments in the temperature range 500–1000 °C. At the temperatures where austenite exists, carbon diffuses from ST1 into ST2; when ferrite is present, the diffusion flow reverses from ST2 into ST1. This effect is attributed to the degree of the silicon influence on the graphite precipitation and carbon activity in ST1 and ST2 steels. The opposite signs of the activity gradients in austenite and ferrite cause the reversal of the carbon diffusion when the annealing temperature is changed from the austenite to the ferrite temperature region. The carbon diffusion coefficients D_C and the thermodynamic interaction coefficients ε_C^Si in austenite have been assessed from the experimental data for ST1 and ST2 steels.     

Mechanical properties of cast lead alloy/silicon carbide particulate composites

This paper describes a study of the mechanical properties of cast lead-antimony alloy composites containing silicon carbide (SiC) particles of size 90–150 μm and of contents ranging from 0% to 5% by weight. The ‘vortex method’ of production was employed in which the SiC particles were poured into the vortex created by stirring the molten metal at 400°C by means of a mechanical agitator. The results of this study revealed that as SiC composition was increased, there were significant increases in the ultimate tensile strength (UTS), hardness, torsional strength and impact strength of the composite, accompanied by a reduction in its ductility. An attempt is made in the paper to provide explanations for these phenomena.     

Aging behaviour of Al–Cu–Mg alloy–SiC composites

The age-hardening kinetics of powder metallurgy processed Al–Cu–Mg alloy and composites with 5, 15 or 25 vol.% SiC reinforcements, subjected to solution treatment at 495 °C for 0.5 h or at 504 °C for 4 h followed by aging at 191 °C, have been studied. The Al–SiC interfaces in composites show undissolved, coarse intermetallic precipitates rich in Cu, Fe, and Mg, with its extent varying with processing conditions. Examination of aging kinetics indicates that the peak-age hardness values are higher, and the time taken for peak aging is an hour longer on solutionizing at 504 °C for 4 h, due to greater solute dissolution. Contrary to the accepted view, the composites have taken longer time to peak-age than the alloy, probably due to lower vacancy concentration, large-scale interfacial segregation of alloying elements, and inadequate density of dislocations in matrix. The composite with 5 vol.% SiC with the lowest inter-particle spacing has shown the highest hardness.     

Reduction of carbon impurities in silicon oxide films prepared by rf plasma-enhanced CVD

Silicon oxide films were deposited at near room temperature by a remote-type radio frequency plasma-enhanced chemical vapor deposition using a mixture of tetramethoxysilane and oxygen as source gas. The temperature of the reactor wall was controlled from 25 to 150°C. Carbon impurities which existed as Si–CH₃ in the deposited films were reduced markedly when the substrate temperature was kept higher than the wall temperature during deposition. The optimum substrate temperature was 50°C to obtain carbon-free silicon oxide films at a wall temperature of 30°C. X-Ray photoelectron spectroscopic analyses of the films proved that carbon impurities existed only on the film surfaces.     

Microstructures and improved wear resistance of 3D needled C/SiC composites with graphite filler

Three-dimensional (3D) needled carbon/carbon (C/C) composites with a lowest porosity of 15.6% were achieved after 1 cycle of impregnation by phenolic resin slurry containing graphite filler, hot-pressing curing and pyrolysis. Carbon/silicon carbide (C/SiC) composites were obtained by liquid silicon infiltrating C/C composites. The aim was to incorporate cost effectiveness and excellent performance of C/SiC braking material. Using filler content not exceeding 30 wt% in the slurry promised undamaged C/C segments in C/SiC composites. The linear wear rate of C/SiC using 30 wt% filler was 0.33 μm side⁻¹ cycle⁻¹ and displayed a fourfold decrease; its weight wear rate was 2.46 mg side⁻¹ cycle⁻¹ and minus 171%, compared with the previously reported values of C/SiC without filler, at a braking velocity of 28 m/s. Its friction coefficients and friction stability coefficients appeared relative insensitive to changes in braking velocities and displayed higher values at high braking velocities compared with the previous values.     

Fabrication of multi-walled carbon nanotube-reinforced carbon fiber/silicon carbide composites by polymer infiltration and pyrolysis process

Multi-walled carbon nanotube (MWNT)-reinforced carbon fiber/silicon carbide (C_f/SiC) composites were prepared using a polymer infiltration and pyrolysis (PIP) process. The MWNTs used in this study were modified using a chemical treatment. The MWNTs were found to be well dispersed in the matrix after ultrasonic dispersion, and the mechanical properties of the C_f/SiC composite were significantly improved by the addition of MWNTs. The addition of 1.5 wt.% of MWNTs to the C_f/SiC composite led to a 29.7% increase in the flexural strength, and a 27.9% increase in the fracture toughness.